HPLC紫外检测法测定辣椒制品中苏丹红I～IV号含量的研究

Determination of Sudan I～IV in Capsicum Foods with UV Detecter and High Performance Liquid Chromatography (HPLC)

实验选用氟罗里硅土(FLORISIL)固相萃取(SPE)柱对样品进行净化,用DIKMA公司C18(150×4.6mm,5μm)钻石柱为色谱柱,以含5%水的乙腈溶液为流动相,以229nm为检测波长,对辣椒食品中的苏丹红I～IV号进行了分离和检测。结果显示:苏丹红I～IV号分别在0.625～2000ng、2.5～2000ng、5～2000ng、5～2000ng范围内呈良好的线性关系,相关系数R2分别为1、1、0.9989和0.9990。其标准回收率分别为100.76%、100.20%、99.86%、100.09%,变异系数分别为1.04%、1.80%、3.29%、3.06%。辣椒粉样品中的苏丹红I～IV号的加样回收率分别为102.14%、103.69%、96.36%和101.93%,变异系数分别为1.49%、0.84%、0.93%和3.64%;辣椒油样品中的苏丹红I～IV号的加样回收率分别为97.03%、100.81%、94.53%和99.31%,变异系数分别为2.85%、1.71%、1.92%和2.79%。苏丹红I～IV号的最低检测限分别为1.88、2.5、6.25和10μg/kg。该方法样品处理简单,灵敏度高,可在有关实验室推广应用。

Objective： This study established a method based on high performance liquid chromatography （HPLC） with solid phase extraction for determining Sudan I-IV in food. Methods： The Sudan I-IV were extracted with N-hexane and purified with FLORISIL solid phase extraction from food, and separated on a C18 column with 5% water of acetonitrile solution as the mobile phase, and detected at 229 nm. Results： The calibration curves of Sudan I-IV show good linearity in the different ranges 0.625-2000 ng （R^2=l）, 2.5-2000 ng （R^2=l）, 5-2000 ng （R^2=0.9989） and 5-2000 ng （R^2=0.9990） respectively. The detection limits of Sudan I-IV are 1.88, 2.5, 6.25 and 10 μg/kg, respectively. The standard recovery rates of Sudan I-IV are 100.76%, 100.20%, 99.86% and 100.09%, respectively. The paprica application of sample recovery rates are 102.14%, 103.69%, 96.36% and 101.93%, respectively. The capsicol application sample recovery rates are 97.03%, 100.81%, 94.53% and 99.31%,respectively. Conclusions： This method is simple, rapid, accurate, reliable and applicable for routine analysis.